Methane → HCID 66733858, 화합물

HRID 1929616노트

반응식

HRID 1929616 반응식
[CH2:1]([O:5][C:6](=[O:18])[CH:7]=[CH:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([CH3:16])=[C:11]([F:17])[CH:10]=1)[CH2:2][CH2:3][CH3:4].C>[Pd].CO>[CH2:1]([O:5][C:6](=[O:18])[CH2:7][CH2:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([CH3:16])=[C:11]([F:17])[CH:10]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 2

HCID 297MethaneHCID 66733998HCID 66733998, 화합물

생성물 1

HCID 66733858HCID 66733858, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 3-(3,5-difluoro-4-methyl-phenyl)-acrylic acid butyl ester (7.651 g; 30.089 mmol) and 10% palladium over activated charcoal (0.760 g) was placed under nitrogen before MeOH (100 ml) was carefully added. The resulting suspension was placed under vacuum, then under hydrogen (1 atm), and the reaction mixture was vigorously stirred at rt for 2 h45. The reaction mixture was filtered over a pad of celite, and concentrated under reduced pressure to give the expected product 3-(3,5-difluoro-4-methyl-phenyl)-propionic acid butyl ester as a yellow oil which was further dried under HV (6.960 g; 90%). LC-MS: tR=1.10 min; [M+H]+: no ionisation.

후처리

  1. additionwas carefully added
  2. filtrationThe reaction mixture was filtered over a pad of celite
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f22a620250634a2eb9b20ad420dd3967
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188082B2

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